Composites Science and Technology 185 (2020) 107890

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Composites Science and Technology

journal homepage: http://www.elsevier.com/locate/compscitech

Thermo-mechanical and morphological characterization of needle punched

non-woven banana fiber reinforced polymer composites
Jack J Kenned a, *, K Sankaranarayanasamy a, b, J.S Binoj c, Suresh Kumar Chelliah d
a
Department of Mechanical Engineering, National Institute of Technology, Tiruchirappalli, 620015, Tamil Nadu, India
b
Department of Mechanical Engineering, National Institute of Technology, Puducherry, 609609, Puducherry, India
c
Department of Mechanical Engineering, Sree Vidyanikethan Engineering College, Tirupati, 517102, Andhra Pradesh, India
d
Department of Aeronautical Engineering, Bharath Institute of Higher Education and Research, Selaiyur, Chennai, 600073, Tamilnadu, India

A R T I C L E I N F O A B S T R A C T

Keywords: The purpose of this study is to employ a novel technique for the fabrication of natural fiber reinforced polymer
banana fiber composites that could stand toe to toe with glass fiber composites in terms of thermo-mechanical properties
Needle-punch without any chemical treatment. The reinforcement fibers were extracted from the pseudostem of the nendran
Polymer composites
banana plant. Later a non-woven fabric composite consisting of banana fibers reinforced with unsaturated
Thermo-mechanical properties
Morphological properties
polyester (UPE) matrix was fabricated using the needle punching technique. Composite specimens were sub­
jected to tensile, flexural, hardness, quasi-static indentation (QSI) and dynamic mechanical analysis (DMA) test
for evaluating mechanical properties. However, the optimal properties was achieved at 40 wt% fiber content
with an increase in tensile and flexural strength of 36% and 33% for needle-punched banana fiber composites
(NPBFC) compared with random banana fiber composites (RBFC) respectively. It was also evidenced from the
load bearing capacity and hardness of NPBFC having 2420 N and 87 HRRW, proves its superiority over RBFC and
comparable with RGFC. Further, the viscoelastic properties of UPE and NPBFC were analyzed. Subsequently, the
characteristic bonds of cellulose were represented through infra-red spectroscopy and the crystallinity index was
exposed through X-ray diffraction analysis. In addition, thermal analysis was done and the stability of the
optimized NPBFC witnessed was up to 260 � C. Also, morphology-properties correlation was established. Finally,
the experimental results were validated using theoretical models. This study concludes that the synthesized novel
NPBFC endorses its potentiality as a probable reinforcement in industrial safety helmet, automotive door panel
and light weight structural applications.

1. Introduction
Any natural or man-made materials capable of being processed into a
fabric can be defined as a fiber. Natural fibers are those which are not
synthetic or man-made but could be sourced from animals or plants [1].
Realizing the insalubrious nature of synthetic fibers, researchers are
currently gingerly turning away from them and focusing on the alter­
native, natural fiber composites (NFCs) [2–4]. Products made using
these fibers have seamlessly made their way into the industry in a
multitude forms [5–10]. Moreover, low density, high specific strength
and stiffness, low cost, less absorption of CO2, less hazardous
manufacturing processes, good electrical resistance, acoustic insulation,
low emissions and less abrasive damage to processing equipment by
NFCs compared to synthetic fiber composites are the advantages that
have further kindled this change [11–13]. However, NFCs are not
exactly problem-free as they pose issues of moisture absorption, lower
strength, greater variation of properties and lower durability [14–16].
Despite these setbacks, bio-degradability and the environmental benefit
characteristics have made natural fibers a popular reinforcement in
polymer matrix which can potentially replace traditional aramid fiber,
carbon fiber and glass fiber composites [17,18].
Various plant fibers that have been explored as a potential rein­
forcement include oil palm, areca, coir, jute, flax, hemp, ramie, kenaf,
coconut, banana, sisal, and pineapple [19,20]. Out of these, banana fi­
bers have been studied extensively [21,22]. India and Brazil are the
largest producers of banana fibers. Production of banana in India during

* Corresponding author.
E-mail addresses: jacknittmech@gmail.com (J.J. Kenned), director@nitpy.ac.in (K. Sankaranarayanasamy), binojlaxman@gmail.com (J.S Binoj), sureshkumar.
aero@bharathuniv.ac.in (S.K. Chelliah).

https://doi.org/10.1016/j.compscitech.2019.107890
Received 8 June 2019; Received in revised form 16 October 2019; Accepted 25 October 2019
Available online 31 October 2019
0266-3538/© 2019 Elsevier Ltd. All rights reserved.
J.J. Kenned et al.
2016–2017 had reached around 29.16 million tones, being cultivated in
an area of 858 ha [23]. Such a large production results in a similar
magnitude of bio-waste and the banana fibers used in the composite
fabrication are extracted from the pseudostem of the banana plant
(Musa sapientum), which is supported by its abundant supply and at no
additional cost [21].
Considerable research has been done on the subject of improvement
of the properties of lignocellulosic fiber composites, which banana fiber
composites fall under. Structural constituents, relative concentrations,
various fiber parameters like length, distribution, diameter and orien­
tation strongly influence the properties of the composite [24]. However,
handling of an effective load transfer between the fiber and matrix re­
quires that the interfacial interactions of the constituents should be
strong [25]. The chemical modifications were adopted for overcoming
this issue and to enable impactful influence on the properties of the
composite. For banana fiber composites, the chemical treatments per­
formed include alkaline, acetylation treatment [26], silane treatment
[27], permanganate, benzoylation treatment [28] and maleated
coupling reagents [29]. However, all these chemical treatments have
their own limitations. Though it improves the interfacial bonding these
are highly toxic, time consuming, costly and polluting the environment
this prompted to study about an alternate method which would elimi­
nate the above said hassles. Hence the objective of this study is to
fabricate a novel needle punched banana fiber reinforced polymer
composites as a potential and alternate replacement for the existing
carcinogenic composites.
However, there is no report seen in literature on the study of un­
treated needle punched non-woven banana fiber composites. In this
study, banana fibers extracted from the Nendran variety of banana
plants were needle-punched to form a non-woven fabric, thereby
bonded with an unsaturated polyester matrix forming a novel NPBFC.
The investigated thermal, mechanical and morphological properties of
NPBFC express its potentiality as a probable reinforcement in industrial
safety helmet, automotive door panel, garden railing and light weight
structural applications.
2. Materials and methods
2.1. Raw fiber extraction from the banana plant
Different varieties of banana plants including Red banana, Nendran,
Rasthaly, Morris and Poovan were analyzed for their physico-chemical
properties by Kiruthika and Veluraja [30]. The present investigation
deals with the nendran variety of banana plant and the selection for this
is on two grounds, is its excellent strength ð� 450 MPaÞ and better
Fig. 1. Flow diagram of composite from plant origin (a) Banana plant (b) Pseudo stem (c) Extracted raw fiber (d) Needle punching machine, (e) Needle punched fiber
roll and (f) NPBFC.
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Composites Science and Technology 185 (2020) 107890
economy compared to the other variety of bananas. The pseudostem was
removed from the mature banana plant; nine days post its harvesting.
From the pseudostem, the cortex region was extracted and fed into the
retting machine to extract the fibers. Subsequently, the extracted fibers
were sun dried for a period of 7–9 days to reduce the moisture content.
Later, these dried fibers were kept in the oven at temperatures ranging
from 50 � C to 60 � C for a period of 12–16 h for removal of the entire
moisture content. These dried fibers were further subjected to a me­
chanical scutching process for easy removal of fibers from any hurds
adhering to the fiber bundles using turbine blades. Fig. 1 represents the
process flow diagram of composite from the plant origin.
2.2. Chemical and physical properties of raw banana fiber
The quantity of holo-cellulose was quantified by D Addico, Wise and
Murphy method. Lignin and α cellulose content were determined by
using TAPPI standards T 222-OM-06 and T 203 respectively [31].
Hemicellulose was calculated by using the following relation
Hemicellulose ¼ (quantity of holo-cellulose - quantity of α cellulose)
The chemical and physical properties of raw banana fiber are listed
in Tables 1 and 2 respectively.
2.3. Botanical properties of raw banana fiber
Narrow and wide banana sheath fibers were individually inspected
by micro technique for the purpose of investigating its interior structure.
The sheath of banana plant was sliced into small pieces and immersed in
FAA solution (Maleic acid 5 ml þ Formaldehyde 5 ml þ 70% ethyl
alcohol of 90 ml) for duration of 24 h for specimen preservation. Later,
they were dried out using tertiarybutyl alcohol and implanted in
paraffin blocks. Further, the blocks were partitioned into a size of 10–12
m pieces by a rotary microtome that revolved in the right-handed di­
rection. The prepared samples were then fixed to a glass slide stained
with safranine and toluidine blue for improvement in image visibility.
Table 1
Bio-chemical properties of raw banana fiber.
Property Quantity
Cellulose (%) 71.08
Hemicellulose (%) 12.61
Lignin (%) 7.67
Moisture (%) 6.73
J.J. Kenned et al. Composites Science and Technology 185 (2020) 107890

Table 2 3.1. Mechanical testing

Physical properties of raw banana fiber.
Property Quantity The fabricated composite specimens were tested for tensile, flexural
and hardness properties as per ASTM standards. Tensile and flexural
Diameter (μm) 138 � 0.0671
Density (g/cm3) 1.28 tests were carried out using UK made Tinius Olsen universal testing
Tensile Strength (MPa) 412.5 � 46.7 machine (UTM) having a 50 kN load cell and a cross head speed of
Elongation at break (%) 27.89 0.5 mm/min adhering to ASTM-D3039 and ASTM-D790 standards
Microfibril angle (� ) 11 respectively. In addition, QSI tests were also performed on the same
Lumen size (μm) 6
UTM using hemispherical indenter with 12.7 mm diameter for evalu­
ating indentation damage resistance of the specimens. Meanwhile,
Finally, the specimens were observed with the help of a polarized light hardness of the composite samples was tested following the ASTM-
micrograph for examining the fiber structure. D785-98 standard using a data acquisition system embedded in a
Rockwell hardness testing machine. In each case, five samples were
tested and considered for calculating standard deviation.
2.4. Needle punching technique
3.2. Thermal analysis of NPBFC
Needle-punching technique was used for mechanical entanglement
of webs or batts of 30 mm long fibers to produce the fabric. This was
Thermal stability of the optimized NPBFC was analyzed by Thermo-
accomplished through the action of reciprocating barbed (felting) nee­
Gravimetric Analysis (TGA) Model 4000 (Germany made). An amount of
dles which interlocked the fibers. The consolidated structure maintained
6–8 mg of the pulverized composite specimen was placed in an alumina
its integrity through inter-fiber friction. A triangular barbed needle of
crucible for testing and the process was carried out in an inert atmo­
regular barb spacing which implied an evenly spacing 9 barbs on a blade
sphere with Nitrogen flowing in at a rate of 20 ml/min. The temperature
of � 30 mm in length was used with an optimized penetration depth of
was increased in steps of 10 � C/min from 35 to 850 � C.
8 mm and a punch density of 100 punches/cm2.
3.3. Dynamic mechanical analysis (DMA)
3. Composite preparations and testing
DMA test was carried out to analyse the viscoelastic properties of
Unsaturated polyester resin, Methyl Ethyl Ketone Peroxide (MEKP) UPE and NPBFC specimens (10 wt % to 50 wt %) as per ASTM D 4065-01
and accelerator cobalt naphthalene were procured from LEO Enter­ standard using DMA Q800 V 7.4 (TA instruments, USA) set up. Single
prises, Nagercoil. Unsaturated polyester was selected as the matrix cantilever clamp, temperature sweep mode was employed to charac­
material, due to its excellent process ability and cross-linking tendency. terize the specimens. The specimens were applied with sinusoidal stress
Later, the matrix was mixed with catalyst Methyl Ethyl Ketone Peroxide of 1 Hz frequency and strain amplitude of 25 μm. The experimentation
(MEKP) and accelerator cobalt naphthalene in a ratio of 98:1:1. The was conducted in the temperature range of 25 � C–170 � C with the
characteristics of the pure resin were tested for physical and mechanical heating rate of 2 C/min.
�

properties are listed as in Table .3. A mild steel mold of dimensions

300 � 150 � 3 mm3 was used for the preparation of the composites with 3.4. Fourier-transform infrared (FTIR) spectroscopy of NPBFC
different fiber wt. %. The NPBF were impregnated with the prepared
resin in the mold and compressed with a lid to form a sheet using the The Optimized NPBFC sample was dried, ground to powder and then
hand lay-up technique. In order to maintain homogeneity in the mixture, pelletized with KBr. Four scans were taken at a resolution of 4 and the
a mechanical stirrer was used and a continuous stirring process was infrared spectrum for the optimized NPBFC sample was obtained using a
performed. During this process, extreme care was taken to avoid PerkinElmer Spectrum 2 series 93947 of version 10.03.09 for the
clumbing and tangling during mixing. Later, the matrix was degassed by wavelength ranging from 400 cm 1 to 4000 cm 1.
hand with the help of a roller and allowed to settle down by applying a
compression load of 350 kN. The entire process was carried out at 3.5. Structural characterization of NPBFC
ambient temperature (�27 � C) with a relative humidity of about 65%.
Silicon spray was applied over the mold for removing the cured NPBFC. Optimized NPBFC was pulverized to obtain a fine powder and
Similarly, procedure was adopted for fabrication of 30 mm RBFC as well compacted at a pressure of 110 MPa. The compacted powder was then
as RGFC specimens. held in a standard disk of the Rigaku Ultima III X-ray Diffractometer for
a continuous scanning mode at a scan speed of 2� /min and temperature
Table 3 of 300 K. The step size adopted for this procedure was 0.02� (2θ) in the
Properties of unsaturated polyester (liquid and cured) resin. angular range of 10� –80� . The sealed-tube of Cu-Kα radiation was
Liquid Resin operated at 40 kV and 32 mA at a wavelength of 1.54 o A for deriving the
Density 1.18 g/cm3 X-ray Diffraction (XRD) patterns of optimized NPBFC.
Appearance Slightly yellow viscous liquid
Acid value 22 � 3 mg KOH/g 3.6. Morphological analysis
Specific gravity at 25 � C 1.25 � 0.04
Viscosity at 25 � C 220-280 cP
Volatile content 35 � 1 wt%
Composite specimens subjected to tensile and flexural testing were
analyzed for surface fracture and fiber matrix inter-relations using
Cured Resin
FESEM images taken by Carl Zeiss Microscope of Model SIGMA, with the
Tensile strength 36.0 � 2 MPa X Flash detector energy resolution above 126eV and an acceleration
Tensile modulus 1.23 � 0.2 GPa
voltage range of 0.21–30 kV. The fractured RBFC, RGFC and NPBFC
Elongation at break 1.32 � 0.25%
Flexural strength 42.10 � 2.51 MPa samples having dimensions 5 mm � 5 mm x 3 mm were taken and
Flexural modulus 1.71 � 0.21 GPa mounted on a specimen stub. Prior to being subjected to imaging, the
Shear strength 4.5 � 0.54 MPa samples went through vacuum sputter coating where they were coated
Impact strength 0.62 � 0.03 J/cm2 with an ultrathin layer of gold for making the surface conductive in
Rockwell hardness 61 � 2 HRRW
order to avoid electron charge accumulation.

3
J.J. Kenned et al.
4. Results and discussion
4.1. Anatomical analysis of banana pseudo stem
The banana leaf sheath consists of an outer ad axial thick portion and
an inner ab axial thin portion with wide air chambers in between the
outer and the inner portions as shown in Fig. 2(a, b). The wide median
chamber is divided by thick vertical partitions. The vertical partitions
have isolated vascular strands and circular masses of fibers. The vascular
strands have wide circular vessels associated with phloem and fibers
surrounding the vascular strands.
In the ad axial and ab axial segments, the leaf sheaths are larger and
smaller with discrete circular fiber bundles Fig. 2(c, d, e and f)
embedded in the walled compact ground parenchyma cells, whereas the
fiber bundles differ in their distribution. The fibers are libri forms type
and have thin lignified walls and wide lumen. The cell lumen of the fiber
wall is 5 μm in wide and 2 μm in thick. However, when the fiber bundle
is macerated, the fibers are either in thick solid bundle or separated into
individual fibers of two types, one as narrow fibers with thin narrow and
gradually tapering towards the ends, and the other as fibers wide with
wide lumen and long tapering towards the ends as shown in Fig. 2(e, f).
The anatomical analysis, it ensured the promotion of better bonding
characteristics by the presence of the fiber bundles with vascular strands
around the cell lumen of the banana leaf sheath when employed as
reinforcement with the polymer matrix during composite fabrication.
Fig. 3 (a, b) show the narrow and wide fibers with a bundle of fiber
extracts embedded in them. The structure of a cell wall consists of four
components, namely, primary wall, secondary wall; middle lamellae and
cell lumen. These are depicted in Fig.3(c–h). The measurement of cell
wall was done using the image processing technique through Image J
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Composites Science and Technology 185 (2020) 107890
software. Details are tabulated in Table .4. The primary wall had cel­
lulose which provides a boost to the strength of the fiber, whereas the
secondary wall had lignin resulting in hardness to the fiber. Moreover,
the middle lamellae is an intercellular layer joining the adjacent cells are
made up of hemicellulose and lignin, whereas the middle part of each
cell comprises free space for storage of water, referred to as lumens.
4.2. Estimation of tensile and flexural strength
Embedding the fibers in the matrix improves the tensile properties of
the composite due to superior inherent strength compared to the matrix
[32]. Fig. 4(a) shows the tensile strength of the UPE, RBFC, RGFC and
NPBFC. When the fibers were embedded in the matrix, a shift in nature
from brittle to ductile was observed. As the fiber wt. % of the RBFC,
RGFC and NPBFC increased from 10 to 40 wt %, an increase in strength
was noticed. Also, when the fiber content was increased beyond 40 wt
%, an abrupt reduction in strength was observed. Significantly the
NPBFC proved its superiority over the RBFC with values approaching
those of the RGFC.
The strength of the pure resin is low due to its brittle nature. At 10 wt
% fiber content, the failure observed was predominantly brittle in nature
which was the result of the presence of higher amount of matrix hence
low strength of the composites. Between 20 and 30 wt % fiber content,
the tensile strength is marginally increased due to a minute improve­
ment in the interfacial bonding between the composite constituents,
whereas the occurrence of failure arising as a result of the brittle failure
of the matrix and a ductile fiber pull-out. However, at 40 wt % fiber
content the best performance was revealed due to optimal interfacial
bonding. The nature of failure occurred was very little brittle failure
largely associated with ductile fiber pull-out as well as fiber-matrix
Fig. 2. Anatomical micrographs of banana plant
pseudo stem: (a) - Transverse section of banana
sheath showing upper horizontal portion and verti­
cal partition, (b) - Transverse section of leaf sheath
showing lower horizontal portion and vertical
partition, (c) - Fiber bundles of leaf sheath, (d) -
Fiber bundles enlarged, (e) - Larger fiber bundles
enlarged and (f) - Smaller fiber bundles along the
epidermal region. [AC - Air Chamber, AbS - Abaxial
Side, Fi- Fiber, Pa - Parenchyma, Ph- Phloem, Ve-
vessel, VaSt & VSt - Vascular Strand, VePa - Vessel
Parenchyma, AdE - Adaxial Epidermis, FiB - Fiber
Bundle, GPa & GP- Ground Parenchyma, Hd- Hypo­
dermis, AbE – Abaxial Epidermis].
J.J. Kenned et al.
debonding. This proves the enhanced stress transfer between the matrix
and fiber. Beyond 40 wt %, a decreasing trend in the tensile strength was
observed. This was due to fiber agglomeration factor which leads to
inefficient stress transfer from matrix to fiber.
The superiority of the NPBFC might be attributed due to the needle-
punching action that might have roughened up the fiber’s surface,
possibly removing unwanted residues like wax from the fibers and
enhancing the interfacial bonding through mechanical interlocking.
Generally, the tensile load applied to a composite is transferred to the
fibers by means of shearing mechanism. A homogeneous mass per unit
area (GSM) was obtained by needle punching technique for all fiber wt.
% of NPBFC samples, due to the possession of a uniform fiber laying
pattern, which led to a smoother stress transfer along the entire speci­
mens unlike what was observed for RBFC and RGFC.
The resin uptake of the NPBFC increases by the use of an optimum
needling density (100 punches/cm2), leading to a better peg formation
and, as a consequence, increase in strength, making the packing of fiber
assembly in an array and thus more compact in nature [33]. When the
punch density is below the optimized level, the fibers are poorly
entangled, if it is above due to the severe action of the barbs fiber
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Composites Science and Technology 185 (2020) 107890
Fig. 3. Optical micrographs of banana plant pseudo
stem: (a) - Fibers separated showing Narrow Fibers
and Wide Fibers, (b) - A bundle of Fibers intact, (c) -
Wide Fiber Tapering part, (d) - Wide Fiber-Middle
part, (e) - Wide Fiber showing Tapering end
portion, (f) - Wide Fiber - Middle part, (g) - Narrow
Fiber - Tapering end part and (h) - Narrow Fiber -
Middle part [FiB - Fiber Bundle, NFi - Narrow Fiber,
WFi - Wide Fiber, CL - Cell Lumen, FiE - Fiber End,
ML - Middle Lamella, MP - Middle part, PW - Primary
Wall, SW - Secondary Wall, Ep- Epidermis].
breakage were visible. Similarly, an increase in the mass per unit area
(GSM) from 10 to 40 wt % fiber resulting in enhanced wetting and resin
holding capacity due to better resin uptake [34]. Increasing the mass per
unit area beyond 40 wt % (i.e. 50 wt%), the high packing factor hinders
the penetration of resin into fibers, leading to a lower resin uptake,
which leads to inefficient interfacial bonding, thereby reduction in
strength was noticed [35]. On the other hand, the optimized depth of
penetration (8 mm) paves the way for the matrix to effectively penetrate
into the fibers, thereby enhancing its strength. When the penetration
depth is below the optimized level the fiber entanglement will become
puffy, if it is more than optimized, fiber breakages were observed. Hence
it can be concluded that the optimized value of the NPBFC was found as
40 wt % fiber content.
Similar to the trend representing the tensile strength, the flexural
strength of pure resin is low owing to its brittle nature as shown in Fig. 4
(b). As the fiber content is increased from 10 to 40 wt % for RBFC and
RGFC, the flexural strength also increased due to a better embodiment of
the reinforcement and higher degree of orientation along with the ma­
trix. However, beyond 40 wt %, a decreasing trend in the flexural
strength was observed. This was due to inferior interfacial bonding.
J.J. Kenned et al. Composites Science and Technology 185 (2020) 107890

Table 4 the optimized NPBF composite specimen was much higher than the
Cell wall dimensions of narrow and wide banana leaf sheath fiber. 40 wt % RBFC, almost identical with that of 40 wt % RGFC as indicated
Description Dimensions (μm) in Fig. 5(e). The maximum load bearing capacity for 40 wt % RGFC and
Banana Stem Wide Fiber NPBFC are similar and is evident by same amount of dent depth and
Middle part of the fiber absorbed energy for 40 wt % NPBFC are depicted in Fig. 5(d, f). After the
Total thickness of the fiber 25
removal of the intender, the dent depth or residual displacement
Total middle lamella 5
Total primary wall 5 observed was comparably low for 40 wt% NPBFC and 40 wt% RGFC. A
Total secondary wall 5 low dent depth indicative of higher load carrying capacity was recorded
Total cell lumen 10 for tested 40 wt % NPBFC and 40 wt % RGFC. On the other hand, the
Tapering part of the fiber remaining fiber percentages of NPBFC and 40 wt % RBFC resulted in
Thickness of the fiber 14
higher dent depths, indicative of lower load bearing strength.
Cell lumen 8
Primary 2
Secondary wall 3 4.4. Measurement of hardness
Middle lamella 1
Banana Stem Narrow fiber
Hardness is the measure of resistance offered by the composite to
Middle part of the fiber
Fiber total thickness 25 indentation, penetration, abrasion and denting. It is gauged by the
Cell lumen 15 Rockwell ‘R’ scale. The higher the value on the scale, higher is the
Primary wall 3 hardness. Low values were observed for pure resin and, when the fiber
Secondary wall 5 weight percentage increased from 10 wt % to 40 wt % for RBFC and
Middle lamella 2
RGFC, an increasing trend in the hardness was found. The maximum
Tapering part of the fiber
Fiber total thickness 15 hardness was measured at 40 wt %. However, beyond 40 wt % fiber
Cell lumen 8 content, the hardness was found to decline due to poor interfacial
Primary wall 2 bonding as seen in Fig. 6. A similar trend was noticed for the NPBFC
Secondary wall 3
specimen for an increase in mass per unit area. However, the peak
Middle lamella 2
hardness value was almost at par with that of RGFC owing to an optimal
interfacial bonding achieved by enhanced wettability, matrix uptake
Moreover, in case of NPBFC, an intermediate flexural strength be­ and penetration.
tween the RBFC and RGFC was noticed. This was closer to that of RGFC.
The increasing trend in flexural strength was observed for an increment 4.5. Thermal analysis of NPBFC
in mass per unit area from 10 to 40 wt %. This could be attributed to
higher wettability, uniform laying pattern, higher mass per unit area and The thermogravimetric (TG) and differential thermogravimetric
a higher resin uptake as a result of optimized needle penetration and (DTG) analysis of the optimized NPBFC specimen are depicted in Fig. 7
punch density [34]. Nevertheless, beyond 40 wt % fiber content a (a). Three pertinent ranges in the analysis were observed; initial range
reduction in the resin uptake was observed. This was the result of poor was noted between the room temperature and 100 � C, where only a
penetration of matrix into the fiber. Hence at 50 wt % the flexural minor weight loss was witnessed owing to loss in moisture content
strength is abruptly reduced. (evaporation) from the hydrophilic cellulose. This moisture content
could have arisen in the form of non-freezing bound water, freezing
bound water and free water [37–39].
4.3. Evaluation of indentation damage resistance The most visible range and the major weight loss occurred in the
temperature range from 260 � C to 380 � C. This major peak observed
The quasi-static indentation study of the prepared composite speci­ could be due to the degradation in alpha cellulose and hemicellulose.
mens which includes the analysis of peak force, dent depth, linear The final range of the disintegration of the chemical elements was at
stiffness and absorbed energy are shown in Fig. 5(a–f). The slope of the 420 � C, where the ultimate deprivation of sample happened. This may
peak force deformation curve prior to the initial load drop provides be attributed to the dilapidation of the most difficult macro-component
linear stiffness [36] of the quasi-anisotropic RBF, RGF and NPBF com­ present in the sample to decompose, viz. lignin [40] and volatization of
posites. Moreover, the inference from the graph was that the stiffness of the matrix. However, the residues may remain stable up to 800 � C since

Fig. 4. (a) Tensile strength Vs Fiber wt. in % (b) Flexural strength Vs Fiber wt. in % of composites.

6
J.J. Kenned et al.
Fig. 5. Indentation damage resistance of (a) Peak force Vs indentation displacement for RBFC (b) Peak force Vs indentation displacement for NPBFC (c) Peak force Vs
indentation displacement for RGFC (d) Dent depth Vs Fiber wt.% (e) Linear stiffness Vs Fiber wt.% (f) Absorbed energy Vs Fiber wt.% of composites.
Fig. 6. Hardness measurement of RBFC, RGFC & NPBFC.
it requires higher temperatures for degradation. The conclusion from the
analysis was that the optimized NPBFC has appreciable thermal stability
up to 260 � C and opens up avenues for it in a wide range application.
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Composites Science and Technology 185 (2020) 107890
4.6. DMA analysis of UPE and NPBFC
Fig. 8(a) shows the storage modulus (E0 ) as a function of temperature
for UPE and NPBFC specimens. It can be inferred that in all the cases,
when the temperature increases the storage modulus keep on
decreasing. When the fibers are impregnated in the matrix, E0 curves
reveal enhanced storage modulus as the weight percentage of fiber is
increased from 10 wt % to 40 wt % which occurs predominantly in the
transition region. This is due to modulus incompatibility between fiber
and matrix and producing superior interfacial bonding [41]. However,
increasing the fiber content beyond 40 wt % due to agglomeration factor
reduction in storage modulus was observed owing to inferior bonding
between the composite constituents [42]. Interestingly it can be
observed that E’ has the tendency to move towards right when the fibers
are impregnated in the matrix and covers large area both rubbery and
glassy region due to tightly packed constituents.
The amount of energy lost as heat due to viscous flow in UPE and
NPBFC specimens are shown in Fig. 8(b). The plotted E00 curves as a
function of temperature in the DMA test replicate similar trend as that of
E0 plot. It can be stated that all the tested specimen attains peak value
due to dissipation of higher amount of mechanical energy and keep on
decreasing while increasing the temperature. The dissipation of energy
causes polymeric material to be soft with greater chain mobility. It was
observed that reinforcement of fibers in UPE results in peak broadening
of E00 curves due to more chain segment and more free volume [43].
The damping factor of UPE and NPBFC specimens are shown in Fig. 8
J.J. Kenned et al. Composites Science and Technology 185 (2020) 107890

Fig. 7. (a) TG and DTG analysis (b) FTIR spectrum (c) XRD pattern of NPBFC at optimum fiber content.

Fig. 8. DMA test results showing viscoelastic behavior of UPE and NPBFC (a) Storage modulus (E0 ) (b) Loss modulus (E00 ) and (c) tan δ

(c). It might be emphasized that tan δ value is keep on increasing as the
temperature is increased from 25 � C it reaches its peak value in the
transition zone. However, further increasing the temperature tan δ value
decreases which is in the rubbery zone. The increase in the glass tran­
sition temperature (Tg) of the NPBFC specimen can be observed from the
compiled curves. Significantly all the NPBFC specimens exhibited lower
damping factor than the UPE. This is attributed due to unfrozen chain
mobility of the polymer.
4.7. FTIR analysis of NPBFC
The infrared spectrum of optimized NPBFC is obtained as shown in
Fig. 7(b). Alkenes, esters, aromatics, ketenes and alcohol, with different
oxygen-containing functional groups are the main constituents of
biomass [44]. The pivotal spectrum exhibited around 3346.7 cm 1 for
O–H stretching absorption, around 2920 cm 1 for C–H stretching ab­
sorption of aliphatic methylene group, around 2246 cm 1 for C– –O

8
J.J. Kenned et al.
stretching absorption, around 1724.2 cm 1 for C– – C benzene stretching
ring, around 1370 cm 1 for COO axisymmetric stretching, bending of
CH, CH2 and CH3 groups, around 1053.3 cm 1 for C–O–C stretching
absorption at the beta- (1–4)- glycosidic linkage in cellulose and around
650-715 cm 1 for C–O in-plane carbonate bending and S–O sulphate
bending [45]. The spectrum bands at 1595 cm 1and 1105 cm 1 are due
to the presence of lignin and cellulose respectively [30]. Hence, the
present study confirms the availability of chemical constituents and
functional groups in the fiber which in turn have boosted the specific
mechanical properties of the fabricated composites.
4.8. Structural analysis of NPBFC
The XRD pattern of the optimized NPBFC is displayed in Fig. 7(c).
The major peak noted at 2θ ¼ 22.66� in the diffractogram clearly in­
dicates the crystalline features of cellulose. The cellulose standard pro­
file was evident from International Centre for Diffraction Data [46].
Apart from this, the existence of one more phase was seen, i.e the
amorphous phase of lignin, which is revealed by the broad straight line.
This is evident of a healthy cellulose content, which duly increases the
mechanical properties. The Crystallinity index was found as 55%. The
crystallinity fraction indicates the lateral packing of cellulose chain
molecules as high in order, which, in turn, exhibits the superior tensile
strength of the NPBFC [30].
4.9. Microstructural analysis
The interface can be regarded as the three-dimensional boundary
between the fiber and matrix. It is highly critical in controlling com­
posite properties, since fiber-matrix interaction occurs through this
interface. This interaction can be possible through three mechanisms:
mechanical coupling or micromechanical interlocking, physical
coupling such as Van Der Waals or electrostatic interaction and chemical
bonding out of these chemical bonding plays vital role. This is sche­
matically represented in Fig. 9.
The fractured interface of FESEM analysis of the experimented ten­
sile, flexural of RBFC, RGFC and NPBFC specimen for various fiber
weight percentages are shown in Figs. 10 and 11. At 10 wt % fiber
content, the micrograph reveals (Fig. 10(a, f, k)), mostly matrix pores
and peeling. This shows that the failure of the composite specimens was
dominated by matrix failure; hence the strength of the composite
specimens was low. However, when the fiber content was increased
from 10 to 30 wt% (Fig. 10(b, c, g, h, l, m)), due to minute enhancement
in interfacial bonding, the failure was mainly in form of fiber pullout
confirming marginal stress transfer from matrix to fiber. This results in
slight increase in strength of the composite specimens.
Meanwhile, at 40 wt % fiber content (Fig. 10(d, i, n)) the matrix
failure was observed to be very meager and debonding is slightly lower
than 30 wt %. Moreover, it is associated with high dominant fiber pull-
out. This phenomenon resulted in superior strength among all wt. % due
Fig. 9. Schematic representation of chemical bonding at fiber/matrix interface.
9
Composites Science and Technology 185 (2020) 107890
to optimal interfacial bonding. Beyond 40 wt % fiber content (i.e. at
50 wt %), Fig. 10(e, j, o) depicted very little matrix failure along with
high interfacial debonding associated with fiber pull-out which is less
than 40 wt % and more than 30 wt %. This resulted abrupt reduction in
strength due to fiber to fiber contact. However the dominancy of matrix
failure observed in micrograph of NPBFC reveals, as the fiber wt. % is
increased from 10 to 40 wt % is keep on reducing and much lower than
RGFC and RBFC. Moreover, in such cases the failure was dominated by
fiber pull-out which was higher than RGFC and RBFC. This proves that
the stress was transferred from matrix to fiber smoothly than RGFC and
RBFC. Thus NPBFC offered superior in strength.
Similarly, FESEM images of flexural composite specimens of RGFC,
RBFC and NPBFC are displayed in Fig. 11(a–o). The micrograph
revealed similar trend as that of fractured tensile composite specimens.
The predominant failure such as fiber pullout, fiber breakage, matrix
fracture, fiber fracture, matrix peeling, matrix crack, matrix pores, fiber-
matrix debonding and broken fibers was observed in Fig. 11(a, b, c, f, g,
h, k, l, m). However, at 40 wt % fiber content, a honey comb structure
was witnessed even after the fracture. This proves excellent bonding of
fiber with matrix that resulted superior strength. Meanwhile, when the
fiber content arises from 40 to 50 wt %, matrix pores were seen. This was
the result of a less amount of matrix and the agglomeration formation.
Hence the strength was reduced.
5. Theoretical modeling of composite
Various theoretical models have been proposed by renowned scien­
tists for the prediction of the randomly oriented short fiber polymer
composite [47]. Among the various projected models, two pertinent
models and their empirical relation were employed for finding the
tensile properties well before start of the manufacture of the composite
material, based on fiber and matrix properties.
(i) Series model:
σm σf
σc ¼ (1)
σ m Vf þ σ f Vm
(ii) Hirsch’s model:
� �
� �� σf σm
σ c ¼ x σ m Vm þ σ f Vf þ ð1 xÞ � (2)
σ m Vf þ σ f Vm
where Vf -Volume fraction of fiber, Vm -Volume fraction of matrix,
σ m -Tensile strength of matrix (N/m2), σ c -Tensile strength of the com­
posite (N/m2), σ f -Tensile strength of fiber (N/m2), x- Parameter con­
stant having values between 0 and 1.
Analytical comparison of the predicted tensile strength of RBFC,
RGFC and NPBFC with the factual experimental data was made for the
validation of the above models. The model results were correlated with
experimental values. The correlation done was in the range up to opti­
mum fiber content range. The term ‘X’ denotes the volume fraction of
the fiber and ‘x’ is a factor which denotes the stress transfer between
matrix and the fiber. Results attained were found to be better when
x ¼ 0.1 which was applied for the fabricated composites [21]. The
empirical as well as theoretical models regression equations for the
manufactured composite can be stated as below.
(i) Experimental Results
RBFC, σc ¼ 0.154X þ 36.48 (3)
RGFC, σc ¼ 0.642X þ 40.61 (4)
NPBFC, σc ¼ 0.521X þ 35.92 (5)
(ii) Series Model
RBFC, σc ¼ 0.676X þ 32.38 (6)
RGFC, σc ¼ 0.817X þ 39.29 (7)
J.J. Kenned et al. Composites Science and Technology 185 (2020) 107890

Fig. 10. FESEM of fractured tensile specimens: RBFC (a, b, c, d & e @ 10 wt%, 20 wt%, 30 wt%, 40 wt% & 50 wt%), RGFC (f, g, h, i& j @ 10 wt%, 20 wt%, 30 wt%,
40 wt% & 50 wt%) and NPBFC (k, l, m, n & o @ 10 wt%, 20 wt%, 30 wt%, 40 wt% & 50 wt%).

attributed to poor interfacial bonding between the fiber and the matrix,
NPBFC, σc ¼ 0.751X þ 36.15 (8) which is reflected in the experimental curve. However, this phenomenon
does not figure in the two models since they have their own limitation,
(iii) Hirsch’s Model namely applicability only for perfectly bonded materials as depicted in
RBFC, σc ¼ 0.981X þ 32.84 (9) Fig. 12(a–c). The conclusion is that the Hirsch’s model is more corre­
lated with the experimental values with better correlation factor (R2)
RGFC, σc ¼ 1.198X þ 39.06 (10) values for the fabricated composites.

NPBFC, σc ¼ 1.099X þ 36.23 (11)

6. Conclusions
Experimentally, addition of fiber beyond the optimum fiber content
(i.e. 40 wt %) makes the composite strength inferior. This could be The fabricated NPBFC laminate exhibited excellent mechanical

10
J.J. Kenned et al. Composites Science and Technology 185 (2020) 107890

Fig. 11. FESEM of fractured flexural specimens: RBFC (a, b, c, d & e @ 10 wt%, 20 wt%, 30 wt%, 40 wt% & 50 wt%), RGFC (f, g, h, i& j @ 10 wt%, 20 wt%, 30 wt%,
40 wt% & 50 wt%) and NPBFC (k, l, m, n & o @ 10 wt%, 20 wt%, 30 wt%, 40 wt% & 50 wt%).

properties at 40 wt % fiber content. This is much superior than RBFC and
comparable with RGFC. The superior properties were attributed due to
optimized needle punching parameters such as depth of penetration
8 mm and punch density of 100 punches/cm2. Similarly, the uniform
GSM obtained through the needle punching technique enables smooth
transfer of stress from matrix to fiber, thereby improving the mechanical
properties of NPBFC. The TGA revealed optimized NPBFC has excellent
thermal stability up to 260 � C, permitting its use in automotive industry,
safety equipment etc. QSI experimentation confirms the high load
bearing capacity of the NPBFC composites. These were endorsed by the
morphological analysis. Hence NPBFC can be a potential and alternate
replacement for existing carcinogenic RGFC in relation to its thermo-
mechanical properties. This needle punching technique obviates the
traditional use of chemicals to enhance the interfacial bonding of natural
fiber composites, keeping the working environment safe from the ill
effects of these hazardous chemicals leading the way to a greener
environment.
Declaration of competing interest
The authors declared the following conflict of interest statement:

11
J.J. Kenned et al.
Fig. 12. Tensile strength prediction of (a) RBFC (b) RGFC &(c) NPBFC using Series and Hirsch’s models.
(i). All authors have participated in (a) analysis and interpretation of
the data; (b) drafting the article or revising it critically for
important intellectual content; and (c) approval of the final
version.
(ii). This manuscript has not been submitted to, nor is under review
at, another journal or other publishing venue.
(iii). The authors have no affiliation with any organization with a
direct or indirect financial interest in the subject matter discussed
in the manuscript.
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://doi.
org/10.1016/j.compscitech.2019.107890.
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